Process for the treatment of filaments, fibres, fabrics and carpets



United States Patent 3,131,037 PRUCESS F63 TAE TREATMENT OF FHJAMENTS, FEBRES, FABRECS AND @ARPETS Max laquet, Rte. de Nice, Carers, France No Drawing. Filed July 12, 1%1, Ser. No. 123,445 Claims priority, application France lnly 13, 19643 18 Claims. (1. 117-1395) This invention relates to a process for the treatment of filaments, fibres, fabrics and carpets.

Attempts have long been made to improve the resistance to wear of carpets and to protect them against soiling caused by use, for example by footwear. Certain improvements have been made but they are not free from criticism.

Attempts have been made to treat filaments or the woven products produced therefrom, with silicic acid in the form of more or less hydrated silica which was deposited by decomposition of a water-soluble silicate, by thermal decomposition or hydrolysis of an ethyl or methyl silicate; in all cases, the silica gel deposited on the fibres underwent rapid changes and the initially favourable effects, which were obtained, were quickly modified and then presented serious disadvantages.

It has also been proposed to treat the fabrics (or the filaments prior to weaving) with suspensions of colloidal silica obtained as particles of very small dimensions (between 0.010 and 0030 Distinct improvements have been observed, but the results obtained are limited by the impossibility of fixing a sufiicient quantity of this ultra-fine silica on the fibres of the fabrics without giving a dusty, rough or stiff appearance to the woven products which, in order to be acceptable (even for small silica quantities) requires the addition of a softening agent or the use of an emulsifier. These are hydrophilic or surface-active products and communicate these properties to the fabrics, at the same time causing known inconveniences. it has also been proposed to treat the carpets with emulsions or solutions of certain synthetic resins. Some pleasing effects are thus obtained but they are insuificient and far from bein entirely satisfactory.

The present invention is concerned with a process, for the treatment of filaments, fibres, fabrics or carpets, which obviates these defects, and also with the chemical solutions or media for the said treatment.

In accordance with the invention, fibres, filaments or fabrics, e.g. carpets, moquettes and velvets are treated with a solution of an alkyl titanate (more especially butyl tanate), in an organic solvent such as trichlorethylene, and then dried at a temperature between 60 and 160 C. The resulting fabrics show a great improvement in the resistance to wear and at the same time a high degree of protection against dry soiling (such as by dust or dirt of various colours).

More particularly, the invention covers solutions and the treatment by means of solutions which contain, in addition to the alkyl titanate, colloidal silica (preferably obtained by the vapour phase combustion of SiCl in a m xture of hydrogen and air) or ethyl or methyl silicate.

Thus, by adding 3% of colloidal silica (obtained as described above) to a by weight solution of butyl titanate in trichlorethylene and after treating fabrics with this solution and drying them, the treated fabrics have a considerably improved resistance to wear and the protection against dry soiling becomes incomparable; furthermore, the fabrics which were hydrophillic prior to treatment become relatively hydrophobic, and this is very favourable.

The eifects obtained are greatly superior to those which are obtained when treatment is carried out with butyl titanate alone or with colloidal silica alone. There is every cause to believe, and observations confirm this, that the addition of colloidal silica (even in very small quantities) plays an important part in modifying the action of the alkyl titanate on the textile fibers; it seems that its polymerization on drying is modified; in addition, the colloidal characteristics of the solution and of the product fixed 0n the fabric are modified considerably in a favourable manner.

The colloidal silica can be partly or completely replaced by ethyl or methyl silicate. The effects obtained, although less satisfactory than those obtained with the silica, is however acceptable, but the solutions are unstable over a period of time and this limits their possibilities of use.

Advantageously, the solution contains 1 to 20% and preferably between 5 and 8% of alkyl titanate, and O to 7%, preferably between 1 and 3%, of colloidal silica or silicate.

Thus, a solution containing 8 to 10% by weight of alkyl titanate (expressed as pure titanate) and 2.5 to 3% of colloidal silica (expressed as SiO gives excellent results, but the exact quantities to be used depend on the fabric or filaments to be treated, the method of treatment used and the secondary results which are desired (such as pliability, softness and rigidity); consequently they must be established for example by experiment.

It is preferred in many cases that the alkyl titanate is butyl titanate but it can be replaced, preferably only in part, by isopropyl, octyl, titanate; certain secondary characteristics can be obtained by adding these titanates to the butyl titanate. Ricinyl or phenyl titanate may also be added.

The best results have been most frequently obtained by using trichlorethylene or perchlorethylene as solvents, but other organic solvents can be used if they are good solvents for the titanic esters employed and if they have no effect on the esters and the fabrics; the choice of the solvent or solvents depends on each particular case.

The alkyl titanate corresponds to the general formula Ti(OR) in which R is an alkyl radical which can be of various molecular weight. Butyl titanate has the formula Ti(OC H and it can be obtained for example by the action of TiCl, on butyl alcohol, followed by a neutralisation and the elimination of the chlorine (in the form of chloride).

The colloidal silica, in spherical particles of very small dimensions (0.010 to 030 is preferably obtained at high temperature by combustion of SiCL, in hydrogen and in the presence of oxygen.

Furthermore, in accordance with the invention the fabrics (or filaments) can be impregnated by soaking; in this case, it is necessary to adjust the concentration of the solution in order to introduce into the fabric or filaments the quantities of alkyl titanate and colloidal silica necessary for a suitable elfect. In general, it is advisable for velvet-pile carpets or velvets to fix 2 to 4% of colloidal silica and 3 to 8% of alkyl titanate.

The treatment may also be carried out by spraying the solution on to the surface of the fabrics to be treated. Experience shows that spraying 400 to 500 cc. of a solution containing 5 to 10% by weight of alkyl titanate and 1 to 3% of colloidal silica per square metre gives satisfactory results. The nature of these solutions causes a suitable penetration and distribution.

The fabrics thus treated, and after use, can be cleaned subsequently by the conventional dry-cleaning method or by soaping without appreciably modifying the characteristics supplied by the treatment according to the invention. In addition, we have established that after or even before this cleaning, these same fabrics can be retreated by spraying with the same solution (or a similar solution of greater or smaller concentration) in order to improve its properties and its protection in certain cases.

This treatment gives excellent results on velvet-pile carpets or wool velours of difierent qualities, but identical and sometimes better effects are obtained on these fabrics made with synthetic acrylic or nylon fibres, jute, fiax, cotton and with ordinary or round rayon yarns, or mixtures of different fibres.

The eifects obtained by the solutions as described above can be completed, as regards other characteristics, by adding to these solutions other constituents capable of supplying or improving the water-repelling effects or the flexibility.

The fabric-treating solutions, as defined above, are new industrial products. The following non-limiting examples further illustrate the present invention.

Example 1 A solution having the following composition:

G. Trichlorethylene 1,000 Butyl titanate (with about 13% Ti) 80 Colloidal silica (0.010 to 0.030) 30 is prepared at room temperature.

This solution is very fiuid and slightly yellowish in colour.

The surface of a white Wool moquette leaving the production line is sprayed with this solution in an amount of 300 g. per square metre. A good penetration of this solution is observed and the fabric is dried in an air dryer at about 90 C .for about 1 hour. 7 By comparing the resistance to wear, using an abrasion meter, on the same moquette before and after the treatment, it is found that the untreated specimen is worn after 2500 revolutions, While the treated specimen is still not completely worn after 30,000 revolutions, which indicates that the resistance to wear (abrasion) has become at least 10 to 12 times greater.

In a test for checking the protection against dry soiling by dust or dirt of various colours (and also black), it is found that after an identical period of time, the entire untreated specimen has become a dirty deep grey in colour, while the treated specimen maintains an appearance similar to that prior to being subjected to the test and its original appearance is almost completely restored when a conventional suction cleaner is passed thereover once.

The treated moquette, after having been subjected to the accentuated soiling as indicated above, was cleaned by the conventional dry-cleaning process and it was found that its properties were still similar, namely, the same results under the wear test and the same protection against dry soiling.

An identical moquette (at the same stage) was cleaned by washing with ordinary soap and its properties remained substantially identical.

Example 2 The following solution is prepared:

G. Trichlorethylene 1,000 Butyl titanate (about 13% Ti) 40 Colloidal silica (as in Example 1) 8 Mixed wool and yarn filaments are soaked for a few minutes at the workroom temperature in the solution according to Example 2, whereupon they are centrifuged and then dried in an air dryer at a temperature in the region of to C.

A moquette is woven from these filaments and it has the characteristics of those obtained according to Example 1 and Example 2, namely, a much improved resistance to wear and a similar protection against dry soiling.

Example 4 The following solution is prepared:

G. Perchlorethylene 1,000 Butyl titanate (13% Ti) 50 Phenyl titanate 20 Colloidal silica (as in Example 1) 1 0 A wool moquette is treated by spraying this solution as in Example 1, using 450 g. of solution per square metre, whereupon the fabric is dried for one hour at a temperature between 100 and C.

A treated moquette is obtained which has the same characteristics as regards resistance to wear and protection against dry soiling as in Example 1, but it is more pliable and has improved water-repelling properties with a better protection against staining caused by coloured aqueous liquids.

I claim:

1. A process for the treatment of fibrous material, comprising the steps of applying to fibrous material a solution of an alkyl titanate of the formula Ti(( )R) wherein R is an alkyl radical, in an organic solvent therefor and having distributed therethrough a substance selected from the group consisting of colloidal silica and esters of silicic acid; and drying the thus treated fibrous material at a temperature between 60 C. and 0, whereby the resistance to wear and dry soiling of the thustreated fibrous material is improved.

2. A process for the treatment of fibrous material, comprising the steps of applying to fibrous material a solution of an alkyl titanate of the formula Ti(OR) wherein R is an alkyl radical, in an organic solvent therefor and having colloidal silica distributed therethrough; and drying the thus treated fibrous material at a temperature between 60 C. and 160 0, whereby the resistance to wear and dry soiling of the thus-treated fibrous material is improved.

3. A process for the treatment of fibrous material, comprising the steps of applying to fibrous material a solution of an alkyl titanate of the formula Ti(OR) wherein R is an alkyl radical, in an organic solvent therefor and having an ester of silicic acid distributed therethrough; and drying the thus treated fibrous material at a temperature between 60 C. and 160 C., whereby the resistance to wear and dry soiling of the thustreated fibrous material is improved.

4. A process for the treatment of fibrous material, comprising the steps of applying to fibrous material a solution of tetrabutyl titanate in an organic solvent therefor and having distributed therethrough a substance selected from the group consisting of colloidal silica and esters of silicic acid; and drying the thus treated fibrous material at a temperature between 60 C. and 160 C., whereby the resistance to wear and dry soiling of the thus-treated fibrous material is improved.

5. A process for the treatment of fibrous material, comprising the steps of applying to fibrous material a solution of an alkyl titanate of the formula Ti(OR) wherein R is an alkyl radical in an organic solvent therefor and having ethyl silicate distributed therethrough; and drying the thus treated fibrous material at a temperature between 60 C. and 160 C., whereby the resistance to wear and dry soiling of the thus-treated fibrous material is improved.

6. A process for the treatment of fibrous material, comprising the steps of applying to fibrous material a solution of an alkyl titanate of the formula Ti(OR) wherein R is an alkyl radical in an organic solvent therefor and having methyl silicate distributed therethrough; and drying the thus treated fibrous material at a temperature between 60 C. and 160 C., whereby the resistance to wear and dry soiling of the thus-treated fibrous material is improved.

7. A process for the treatment of fibrous material, comprising the steps of applying to fibrous material a solution of an alkyl titanate of the formula Ti(OR) wherein R is an alkyl radical in an organic solvent therefor selected from the group consisting of trichloroethylene and perchloroethylene, and having distributed therethrough a substance selected from the group consisting of colloidal silica and esters of silicic acid; and drying the thus treated fibrous material at a temperature between 60 C. and 160 C., whereby the resistance to wear and dry soiling of the thus-treated fibrous material is improved.

8. A process for the treatment of fibrous material, comprising the steps of applying to fibrous material a solution of between and 8 parts by weight of an alkyl titanate of the formula Ti(OR) wherein R is an alkyl radical in an organic solvent therefor and having distributed therethrough between 1 and 3 parts by weight of a substance selected from the group consisting of colloidal silica and esters of silicic acid; and drying the thus-treated fibrous material at a temperature between 60 C. and 160 C., whereby the resistance to wear and dry soiling of the thus-treated fibrous material is improved.

9. A process for the treatment of fibrous material such as fibers, fabrics, carpets and the like, comprising the steps of applying to said fibrous material a treating liquid consisting essentially of between 5 and 8% by weight of an alkyl titanate of the formula Ti(OR) wherein R is an alkyl radical, between 1 and 3% by weight of a substance selected from the group consisting of colloidal silica and esters of silicic acid, the balance being constituted by an organic solvent for said alkyl titanate; and drying the thus-treated fibrous material at a temperature between 60 C. and 160 C., whereby the resistance to wear and dry soiling of the thus-treated fibrous material is improved.

10. A process according to claim 9 wherein said treating liquid is applied in an amount of between about 300 and 500 grams per square meter of the material to be treated.

11. A process for the treatment of fibrous material such as fibers, fabrics, carpets and the like, comprising the steps of spraying said fibrous material with a treating liquid consisting essentially of between 5 and 8% by weight of an alkyl titanate of the formula Ti(OR) wherein R is an alkyl radical, between 1 and 3% by weight of a substance selected from the group consisting of colloidal silica and esters of silicic acid, the balance being constituted by an organic solvent for said alkyl titanate; and drying the thus-treated fibrous material at a temperature between 60 C. and 160 C., whereby the resistance to wear and dry soiling of the thus-treated fibrous material is improved.

12. A process for the treatment of fibrous material such as fibers, fabrics, carpets and the like, comprising the steps of immersing said fibrous material in a treating liquid consisting essentially of between 5 and 8% by weight of an alkyl titanate of the formula Ti(OR) wherein R is an alkyl radical, between 1 and 3% by weight of a substance selected from the group consisting of colloidal silica and esters of silicic acid, the balance being constituted by an organic solvent for said alkyl titanate; and drying the thus-treated fibrous material at a temperature between 60 C. and C., whereby the resistance to wear and dry soiling of the thus-treated fibrous material is improved.

13. A treating liquid for the treatment of fibrous material, said treating liquid consisting essentially of an organic solvent having dissolved therein an alkyl titanate of the formula Ti(OR) wherein R is an alkyl radical, and having distributed therethrough a substance selected from the group consisting of colloidal silica and esters of silicic acid.

14. A treating liquid for the treatment of fibrous material, said treating liquid consisting essentially of between 5 and 8% by weight of an alkyl titanate of the formula Ti(OR) wherein R is an alkyl radical, between 1 and 3% by weight of a substance selected from the group consisting of colloidal silica and esters of silicic acid, the balance being constituted by an organic solvent for said alkyl titanate.

15. A treating liquid for the treatment of fibrous material, said treating liquid consisting essentially of between 5 and 8% by weight of an alkyl titanate of the formula Ti(OR) wherein R is an alkyl radical said alkyl titanate being selected from the group consisting of butyl titanate, isopropyl titanate and octyl titanate, between 1 and 3% by weight of a substance selected from the group consisting of colloidal silica and esters of silicic acid, the balance being constituted by an organic solvent for said alkyl titanate.

16. A treating liquid for the treatment of fibrous material, said treating liquid consisting essentially of between 5 and 8% by weight of an alkyl titanate of the formula Ti(OR) wherein R is an alkyl radical said alkyl titanate being selected from the group consisting of butyl titanate, isopropyl titanate and octyl titanate, between 1 and 3% by weight of a substance selected from the group consisting of colloidal silica and esters of silicic acid, the balance being constituted by a substance selected from the group consisting of trichloroethylene and perchloroethylene as an organic solvent for said alkyl titanate.

17. A fibrous material resistant to wear and dry soiling, consisting essentially of a fibrous structure at least partially coated with an intimate mixture of the polymerization product of an alkyl titanate of the formula Ti(OR) wherein R is an alkyl radical, and of colloidal silica.

18. A fibrous material resistant to wear and dry soiling, consisting essentially of a fibrous structure at least partially coated with an intimate mixture of between about 5 and 8 parts by weight of the polymerization product of an alkyl titanate of the formula Ti(OR) wherein R is an alkyl radical, and between about 1 and 3 parts by weight of colloidal silica.

References Cited in the file of this patent UNITED STATES PATENTS 1,809,755 King et al. June 9, 1931 2,622,307 Cogovan et al. Dec. 23, 1952 2,628,170 Green Dec. 10, 1953 2,734,835 Florio et al Feb. 14, 1956 2,768,909 Haslam Oct. 30, 1956 2,877,142 Rusher et al. Mar. 10, 1959 2,999,774 Schappel Sept. 12, 1961 OTHER REFERENCES Industrial and Engineering Chemistry, October 1949, 

1. A PROCESS FOR THE TREATMENT OF FIBROUS MATERAIL, COMPRISING THE STEPS OF APPLYING TO FIBROUS MATERIAL A SOLUTION OF AN ALKYL TITANATE OF THE FORMULA TI(OR)4 WHEREIN "R" IS AN ALKYL RADIAL, IN AN ORGANIC SOLVENT THEREFOR AND HAVING DISTRIBUTED THERETHROUGH A SUBSTANCE SELECTED FROM THE GROUP CONSISTING OF COOLOIDAL SILICA AND ESTERS OF SILICIC ACID; AND DRYING THE THUS TREATED FIBROUS MATERIAL AT A TEMPERATURE BETWEEN 60*C. AND 160*C., WHEREBY THE RESISTANCE TO WEAR AND DRY SOILING OF THE THUSTREATED FIBROUS MATERIAL IS IMPROVED. 